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Triethylamine → 2-Allyloxy-4-fluoro-phenylamine

HRID 450037
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HRID 450037 반응식
O.[Sn](Cl)Cl.[CH2:5]([O:8][C:9]1[CH:14]=[C:13]([F:15])[CH:12]=[CH:11][C:10]=1[N+:16]([O-])=O)[CH:6]=[CH2:7].C(N(CC)CC)C>C(OCC)(=O)C>[CH2:5]([O:8][C:9]1[CH:14]=[C:13]([F:15])[CH:12]=[CH:11][C:10]=1[NH2:16])[CH:6]=[CH2:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 197026902-(Allyloxy)-4-fluoro-1-nitrobenzeneHCID 43835034Tin dichloride dihydrate

생성물 1

HCID 624927772-Allyloxy-4-fluoro-phenylamine수율 50%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

Tin (II) chloride hydrate (8.5 g, 38 mmol, 5 eq) was added to a solution of 2-allyloxy-4-fluoro-1-nitro-benzene (1.5 g, 7.6 mmol) in ethyl acetate (20 ml) at room temperature and the mixture was stirred for 4 hr. The reaction mixture was neutralized with triethylamine and then partitioned between water and ethyl acetate. The organic layer was separated, dried over anhydrous sodium sulfate, filtered and concentrated to dryness to give 2-allyloxy-4-fluoro-phenylamine (0.6 g, 50%). The crude compound was used in the next stage without purification.

후처리

  1. custompartitioned between water and ethyl acetate
  2. customThe organic layer was separated
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-a9b68709ee2b4a5e981bc621a46a9ebf
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08486962B2

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